CN106018648B - A kind of method for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy - Google Patents
A kind of method for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy Download PDFInfo
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- CN106018648B CN106018648B CN201610550835.3A CN201610550835A CN106018648B CN 106018648 B CN106018648 B CN 106018648B CN 201610550835 A CN201610550835 A CN 201610550835A CN 106018648 B CN106018648 B CN 106018648B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The present invention discloses a kind of method for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy, through preparing 12 kinds of mycotoxin mixing mother liquors, preparing standard working solution, prepare sample solution, carry out liquid chromatogram-triple tandem quadrupole mass spectral analysis, draw standard curve and result of calculation and complete to detect the concentration of 12 kinds of mycotoxins in the tobacco leaf that goes mouldy.The present invention can be carried out qualitative and quantified to 12 kinds of mycotoxins in the tobacco leaf that goes mouldy exactly, can effectively remove interference of the complex matrices to detection signal, while do not influence 12 kinds of mycotoxin analog values.The inventive method stability is good, accurately and reliably, high sensitivity, simple and quick, reproducible, is especially suitable for complex matrices and goes mouldy the analyses of 12 kinds of mycotoxins in tobacco leaf.
Description
Technical field
The invention belongs to mycotoxin constituent analysis determination techniques field in the tobacco leaf that goes mouldy, and in particular to one kind uses liquid phase
The method that chromatogram-tandem mass spectrometry detects 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy.
Background technology
Storage, fermentation and ageing of the tobacco leaf after redrying are referred to as alcoholization process, and alcoholization process is the important of production of cigarettes
Link, directly affect the quality of cigarette.During alcoholization, usually there is tobacco mildew phenomenon, after going mouldy tobacco leaf can become mildewed,
Paleness is black, tacky, thinning, smelly etc., causes substantial amounts of tobacco leaf to turn into rubbish, larger economic loss is caused to tobacco enterprise.
Tobacco mildew is mainly that microbiology class fermentation causes, and wherein mycotoxin is the secondary metabolite of fungi, can be to mammal
Acute or chronic toxicity is produced, carcinogenic, teratogenesis is partly had been shown to have, causes " three cause " effect of cell mutation.
Therefore, the situation of mycotoxin content in the tobacco leaf that goes mouldy is analyzed, helps to explore fungi growth in the process
Changing rule, provide data for the growth of effective prevention and control microorganism and support, existing detection method is divided into rapid screening method and confirmation method
Two major classes.Rapid screening method is mainly ELISA, and the method has and certain false positive be present, it is impossible to as finally really
Card method.The confirmation method of mycotoxin detection has thin-layer chromatography chromatography（TIC）, liquid chromatography（HPLC）, gas-chromatography
Method（GC）And liquid phase tandem mass spectrometry（LC-MS/MS）Deng.LC-MS/MS can provide simultaneously target compound retention time and
Molecular structure information, has that impurity effect is small, requires purification low, high sensitivity, is adapted to the features such as Simultaneous Analysis for Multicomponent.
Therefore, based on LC-MS/MS qualitative, quantitative advantage, explore exploitation use the triple level Four bars of liquid chromatography-tandem
The method that mass spectrograph determines mycotoxin content in the tobacco leaf that goes mouldy, have to the accurate mycotoxin detected in the tobacco leaf that goes mouldy important
Meaning.
The content of the invention
Gone mouldy for accurate detection the content of mycotoxin in tobacco leaf, the present invention provide a kind of detection go mouldy in tobacco leaf 12 kinds it is mould
The method of verticillium toxin concentration, 12 kinds of mycotoxin concentrations in the tobacco leaf that gone mouldy with accurate qualitative and quantitative detection.
The present invention is achieved through the following technical solutions：A kind of method for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy,
By following each step：
（1）Prepare 12 kinds of mycotoxin mixing mother liquors：It is bent that Penicillium citrinum toxin, deoxidation blood corruption reaping hook mykol, handle are weighed respectively
Mycin, Citreoviridin, T-2 toxin, Aflatoxins M1, fumonisin B2, fumonisin B1, aflatoxin mix target mark
Quasi- product, respectively using methanol dissolving and constant volume, then respectively pipette the above-mentioned 12 kinds of solution of 1 mL in 25 mL respectively in 10mL volumetric flasks
In volumetric flask, using methanol constant volume, 12 kinds of mycotoxin mixing mother liquors are obtained；1ml standard liquids are taken in 25mL volumetric flasks, and
Using methanol constant volume, inner mark solution is obtained；
（2）Prepare standard working solution：0.02 mL, 0.05 mL, 0.10 mL, 0.50 mL and 1.0 mL steps are pipetted respectively
Suddenly（1）12 kinds of mycotoxin mixing mother liquors of gained in 10 mL volumetric flasks, add inner mark solution 1.0mL, use volumetric concentration for
0.1% aqueous formic acid carries out constant volume, obtains standard working solution series；
（3）Prepare sample solution：The tobacco sample to be measured that goes mouldy that 1.0 g are ground is weighed, is placed in 50 mL centrifuge tubes, adds
Enter 20 mL Extraction solvent A, vortex 1min, mechanical shaking extraction 60min, then with 5000rpm rotating speed centrifugation 5min after, by supernatant
It is transferred in another 50mL centrifuge tube, 20mL Extraction solvent B, vortex 1min is then added into residue, continues mechanical shaking extraction
30min, 5min is then centrifuged under 5000rpm rotating speed, merge first time supernatant；In the supernatant that merging is extracted twice
When, precipitation may be produced, therefore, 5 min is centrifuged in 5000rpm rotating speed again, takes 980 μ L end extract solutions（Supernatant）In
In sample bottle, 20 μ L inner mark solutions are added, fully mixes, sample solution is obtained after 0.22 μm of filter membrane；
（4）Carry out the triple level Four bar mass spectral analyses of liquid chromatography-tandem：Using the triple level Four bar matter of liquid chromatography-tandem
Analyzer is composed, liquid chromatogram, the Mass Spectrometry Conditions for analyzing detection are as follows：
Chromatographic column is Waters Acquity BEH C18（1.7 μm, 2.1mm × 100mm）, column temperature：25℃；Mobile phase A
For the aqueous formic acid of volumetric concentration 0.1%, Mobile phase B is the formic acid methanol solution of volumetric concentration 0.1%（Solute is formic acid, molten
Agent is methanol）；Gradient elution, condition are 0 ~ 0.5 min：70% A, 0.5 ~ 10 min：70% A ~ 0% A, 10.0 ~
10.1 min：0% A ~ 70% A, 10.1 ~ 14 min：70% A；Flow velocity：0.2 mL/min, the μ L of sampling volume 5；
Ion gun：Using electron spray ionisation source；Scan mode：Cation scans；Detection mode：Multiple-reaction monitoring MRM；Electricity
Spray voltage：500 V；Dry temperature degree：325℃；Dry gas stream amount：6 L/min；Sheath temperature degree：380℃；Sheath throughput：10
L/min；Capillary voltage：4000 V；
（5）Draw standard curve and result of calculation：Aspiration step respectively（2）It is each in the standard working solution series of preparation
Various concentrations solution carries out LC-MS/MS analyses, in step（4）Under the instrument parameter of determination, with 12 kinds of mycotoxin quota ions
Peak area carries out linear regression to the mass concentration corresponding to it, obtains the standard working curve of each target compound；Draw again
Step（3）The sample solution of preparation carries out LC-MS/MS analyses, in step（4）Under the instrument parameter of determination, 12 kinds of moulds are obtained
Toxin quota ion peak area, regression equation is substituted into, the concentration of 12 kinds of mycotoxins in sample solution is calculated.
The step（1）Aflatoxin mix mark be by aflatoxin B1, aflatoxin B 2, aflatoxin
G1, aflatoxin G 2 form.
The step（1）Standard liquid be containing internal standard substance13C34Fumonisin B1 and13C17Aflatoxin B1
Solution,13C34Fumonisin B1 and13C17The concentration of aflatoxin B1 is respectively 20 μ g/mL.
The step（1）In methanol be chromatographically pure.
The step（3）Extraction solvent A be acetonitrile：The volume ratio of water is 80：20 mixed solution, and add formic acid extremely
Formic acid volumetric concentration is 0.1%.
The step（3）Extraction solvent B be acetonitrile：The volume ratio of water is 20：80 mixed solution, and add formic acid extremely
Formic acid volumetric concentration is 0.1%.
Deionized water of the present invention reaches the requirement of one-level water in GB/T 6682.
The inventive method has advantages below：
（1）The present invention establishes a kind of liquid chromatogram-triple quadrupole bar tandem mass spectrometer while detected 12 in the tobacco leaf that goes mouldy
The method of kind mycotoxin, 12 kinds of mycotoxins in the tobacco leaf that goes mouldy can be carried out exactly qualitative and quantitative.The inventive method
Accurately and reliably, high sensitivity, complex matrices is especially suitable for and are gone mouldy the analyses of 12 kinds of mycotoxins in tobacco leaf.
（2）The present invention uses opposed polarity solvent（Because the volume ratio of acetonitrile/water in Extraction solvent A, B is respectively 80/
20th, 20/80, there is polarity difference in acetonitrile and water, then Extraction solvent A and B have polarity difference, be that two kinds of opposed polarity are molten
Agent）Repeatedly extraction, can effectively remove interference of the complex matrices to detection signal, while it is corresponding not influence 12 kinds of mycotoxins
Value.
（3）The present invention uses BEH C18 chromatographic columns and the selection pair of the formic acid methanol as mobile phase of 0.1% aqueous formic acid+0.1%
The separation of 12 kinds of mycotoxins has reached excellent separating effect.
（4）Deoxidation blood corruption reaping hook mykol detection limit of the present invention is 5.7 μ g/kg, and remaining 11 kinds of mycotoxin detection limit exists
Between the μ g/kg of 0.08 μ g/kg ~ 1.40, withinday precision RSD（n=3）1.31% ~ 8.92%, day to day precision RSD（n=3）
4.80% ~ 12.09%, stability is good, and for the rate of recovery between 78.0% ~ 118.5%, accuracy is high；Liquid chromatography-tandem is triple
Level Four bar mass spectrograph is simple and quick, accurately and reliably, it is reproducible.
Brief description of the drawings
Fig. 1 is that the MRM of Penicillium citrinum toxin quota ion schemes；
Fig. 2 is that the MRM of deoxidation blood corruption reaping hook mykol quota ion schemes；
Fig. 3 is that the MRM of aflatoxin B1 quota ion schemes；
Fig. 4 is that the MRM of the quota ion of aflatoxin B 2 schemes；
Fig. 5 is that the MRM of sterigmatocystin quota ion schemes；
Fig. 6 is that the MRM of aflatoxin G 1 quota ion schemes；
Fig. 7 is that the MRM of Aflatoxins M1 quota ion schemes；
Fig. 8 is that the MRM of the quota ion of aflatoxin G 2 schemes；
Fig. 9 is that the MRM of Citreoviridin quota ion schemes；
Figure 10 is that the MRM of T-2 toxin quota ions schemes；
Figure 11 is that the MRM of fumonisin B2 quota ions schemes；
Figure 12 is that the MRM of fumonisin B1 quota ions schemes；
Figure 13 is13C34The MRM figures of fumonisin B1 quota ions；
Figure 14 is13C17The MRM figures of aflatoxin B1 quota ion；
Figure 15 is that the MRM of certain tobacco leaf aflatoxin B1 quota ion that goes mouldy schemes；
Figure 16 is that the MRM of certain quota ion of tobacco leaf aflatoxin G 2 that goes mouldy schemes.
Embodiment
The present invention is further described below by embodiment.
Prepare determining instrument and material：The triple level Four bar mass spectrographs of liquid chromatography-tandem（Agilent 1290-6460 are beautiful
State）；Assay balance（Plum Teller AB204-S, Switzerland）；Volumetric flask, 10mL, 100mL, conical flask, 50mL；Deionized water（Reach
The requirement of one-level water in GB/T 6682）；Ammonium acetate（Analyze pure, Xilong Chemical Co., Ltd）；Methanol（Chromatographically pure,
Dikma companies）；Formic acid（Analyze pure, Xilong Chemical Co., Ltd）；High pure nitrogen（Purity >=99.999%, Kunming plum plug
That gas products Co., Ltd）
（1）Prepare 12 kinds of mycotoxin mixing mother liquors：It is bent that Penicillium citrinum toxin, deoxidation blood corruption reaping hook mykol, handle are weighed respectively
The mixed mark of mycin, Citreoviridin, T-2 toxin, Aflatoxins M1, fumonisin B2, fumonisin B1, aflatoxin（Contain
There are aflatoxin B1, aflatoxin B 2, aflatoxin G 1, aflatoxin G 2）Standard items in 10mL volumetric flasks,
Respectively use methanol（Chromatographically pure）Simultaneously constant volume is dissolved, then respectively the above-mentioned 12 kinds of solution of 1 mL is pipetted respectively in 25 mL volumetric flasks, adopts
Use methanol（Chromatographically pure）Constant volume, obtain 12 kinds of mycotoxin mixing mother liquors；1ml standard liquids are taken in 25mL volumetric flasks, and are adopted
Use methanol（Chromatographically pure）Constant volume, obtain inner mark solution；Wherein standard liquid is containing internal standard substance13C34Fumonisin B1 and13C17
The solution of aflatoxin B1,13C34Fumonisin B1 and13C17The concentration of aflatoxin B1 is respectively 20 μ g/mL；
（2）Prepare standard working solution：0.02 mL, 0.05 mL, 0.10 mL, 0.50 mL and 1.0 mL steps are pipetted respectively
Suddenly（1）12 kinds of mycotoxin mixing mother liquors of gained in 10 mL volumetric flasks, add inner mark solution 1.0mL, use volumetric concentration for
0.1% aqueous formic acid carries out constant volume, obtains standard working solution series；
（3）Prepare sample solution：The tobacco sample to be measured that goes mouldy that 1.0 g are ground is weighed, is placed in 50 mL centrifuge tubes, adds
Enter 20 mL Extraction solvent A, vortex 1min, mechanical shaking extraction 60min, then with 5000rpm rotating speed centrifugation 5min after, by supernatant
It is transferred in another 50mL centrifuge tube, 20mL Extraction solvent B, vortex 1min is then added into residue, continues mechanical shaking extraction
30min, 5min is then centrifuged under 5000rpm rotating speed, merge first time supernatant；In the supernatant that merging is extracted twice
When, precipitation may be produced, therefore, 5 min is centrifuged in 5000rpm rotating speed again, takes 980 μ L end extract solutions（Supernatant）In
In sample bottle, 20 μ L inner mark solutions are added, fully mixes, sample solution is obtained after 0.22 μm of filter membrane；
Wherein, Extraction solvent A is acetonitrile：The volume ratio of water is 80：20 mixed solution, and formic acid is added to formic acid volume
Concentration is 0.1%；Extraction solvent B is acetonitrile：The volume ratio of water is 20：80 mixed solution, and it is dense to formic acid volume to add formic acid
Spend for 0.1%；
（4）Carry out the triple level Four bar mass spectral analyses of liquid chromatography-tandem：Using the triple level Four bar matter of liquid chromatography-tandem
Analyzer is composed, liquid chromatogram, the Mass Spectrometry Conditions for analyzing detection are as follows：
Chromatographic column is Waters Acquity BEH C18（1.7 μm, 2.1mm × 100mm）, column temperature：25℃；Mobile phase A
For the aqueous formic acid of volumetric concentration 0.1%, Mobile phase B is the formic acid methanol solution of volumetric concentration 0.1%（Solute is formic acid, molten
Agent is methanol）；Gradient elution, condition are 0 ~ 0.5 min：70% A, 0.5 ~ 10 min：70% A ~ 0% A, 10.0 ~
10.1 min：0% A ~ 70% A, 10.1 ~ 14 min：70% A；Flow velocity：0.2 mL/min, the μ L of sampling volume 5；
Ion gun：Using electron spray ionisation source；Scan mode：Cation scans；Detection mode：Multiple-reaction monitoring MRM；Electricity
Spray voltage：500 V；Dry temperature degree：325℃；Dry gas stream amount：6 L/min；Sheath temperature degree：380℃；Sheath throughput：10
L/min；Capillary voltage：4000 V；
The quasi-molecular ion peak of 12 kinds of mycotoxins and 2 kinds of internal standard substances（[M+H]+Quasi-molecular ions）, taper hole voltage, it is quantitative from
Sub, qualitative ion, collision energy（CE）Referring to table 1,12 kinds of mycotoxin standard items and with 2 kinds of each quota ions of internal standard substance
MRM figures are shown in Fig. 1 to Figure 14.
[M+H]+quasi-molecular ions, taper hole voltage, quota ion, qualitative ion, the collision energy of 1 each compound of table
（5）Draw standard curve and result of calculation：Aspiration step respectively（2）It is each in the standard working solution series of preparation
Various concentrations solution carries out LC-MS/MS analyses, in step（4）Under the instrument parameter of determination, with 12 kinds of mycotoxin quota ions
Peak area carries out linear regression to the mass concentration corresponding to it, obtains the standard working curve of each target compound；Draw again
Step（3）The sample solution of preparation carries out LC-MS/MS analyses, in step（4）Under the instrument parameter of determination, 12 kinds of moulds are obtained
Toxin quota ion peak area, regression equation is substituted into, the concentration of 12 kinds of mycotoxins in sample solution is calculated.
Following Method validation is done to the inventive method：Calculate the test limit of this method respectively with 3 times and 10 times of levels of noise
And quantitative limit.The related data of gained is shown in Table 2.
The linear equation of 2 12 kinds of mycotoxins of table, coefficient correlation, test limit, quantitative limit
Certain tobacco sample that goes mouldy is selected, testing result is does not contain 12 kinds of mycotoxins after pre-treatment, therefore is used as empty
White sample, 12 kinds of mycotoxin hybrid standard mother liquors for then adding high, medium and low three contents levels respectively carry out mark-on reclaims
Experiment, calculate the rate of recovery；The withinday precision and day to day precision measure of this method are carried out simultaneously, with the relative mark of measurement result
Quasi- deviation（RSD）Represent, be shown in Table 3.
The withinday precision of 3 12 kinds of mycotoxins of table, day to day precision, the rate of recovery
Sample determines：Scheme from the MRM of testing sample（Figure 15 and Figure 16）In it can be seen that sample in 4.882 min and
There is a chromatographic peak close with the retention time of aflatoxin B 2 and aflatoxin G 2 at 4.746 min, sample is in M/Z=
Characteristic molecular quasi-molecular ions at 258.9 is identical with the characteristic molecular quasi-molecular ions of aflatoxin B 2；Sample is at M/Z=313.0
Characteristic molecular quasi-molecular ions, it is identical with the characteristic molecular quasi-molecular ions of aflatoxin G 2, it may be determined that to contain aflatoxin in sample
B2 and aflatoxin G 2.
The peak area of aflatoxin B in sample 2 and aflatoxin G 2 is substituted into equation of linear regression, you can obtain
The concentration of aflatoxin B 2 and aflatoxin G 2 is 0.446 ng/mL and 2.60 ng/mL in sample, multiplied by with constant volume body
Product, divided by weigh, obtain：This goes mouldy containing the μ g/kg of aflatoxin B 2 7.22, the μ g/ of aflatoxin G 2 42.11
kg。
Claims (4)
- A kind of 1. method for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy, it is characterised in that pass through following each step：（1）Prepare 12 kinds of mycotoxin mixing mother liquors：Penicillium citrinum toxin, deoxynivalenol, handle aspergillus are weighed respectively Element, Citreoviridin, T-2 toxin, Aflatoxins M1, fumonisin B2, fumonisin B1, aflatoxin mix target standard Product, respectively using methanol dissolving and constant volume, then respectively pipette the above-mentioned 12 kinds of solution of 1 mL and held in 25 mL respectively in 10mL volumetric flasks In measuring bottle, using methanol constant volume, 12 kinds of mycotoxin mixing mother liquors are obtained；1ml standard liquids are taken in 25mL volumetric flasks, and are adopted With methanol constant volume, inner mark solution is obtained；（2）Prepare standard working solution：0.02 mL, 0.05 mL, 0.10 mL, 0.50 mL and 1.0 mL steps are pipetted respectively （1）12 kinds of mycotoxin mixing mother liquors of gained in 10 mL volumetric flasks, add inner mark solution 1.0mL, use volumetric concentration for 0.1% aqueous formic acid carries out constant volume, obtains standard working solution series；（3）Prepare sample solution：The tobacco sample to be measured that goes mouldy that 1.0 g are ground is weighed, is placed in 50 mL centrifuge tubes, adds 20 ML Extraction solvent A, vortex 1min, mechanical shaking extraction 60min, then with 5000rpm rotating speed centrifugation 5min after, supernatant is transferred to In another 50mL centrifuge tube, 20mL Extraction solvent B, vortex 1min are then added into residue, continues mechanical shaking extraction 30min, Then 5min is centrifuged under 5000rpm rotating speed, merges first time supernatant；5 min are centrifuged in 5000rpm rotating speed again, 980 μ L end extract solutions are taken in sample bottle, 20 μ L inner mark solutions is added, fully mixes, sample is obtained after 0.22 μm of filter membrane Solution；The Extraction solvent A is acetonitrile：The volume ratio of water is 80：20 mixed solution, and formic acid is added to formic acid volumetric concentration For 0.1%；Extraction solvent B is acetonitrile：The volume ratio of water is 20：80 mixed solution, and add formic acid to formic acid volumetric concentration and be 0.1%；（4）Carry out the triple level Four bar mass spectral analyses of liquid chromatography-tandem：Using liquid chromatography-tandem triple level Four bar mass spectrums point Analyzer, liquid chromatogram, the Mass Spectrometry Conditions for analyzing detection are as follows：Chromatographic column is Waters Acquity BEH C18,1.7 μm, 2.1mm × 100mm, column temperature：25℃；Mobile phase A is volume The aqueous formic acid of concentration 0.1%, Mobile phase B are the formic acid methanol solution of volumetric concentration 0.1%；Gradient elution, condition be 0 ~ 0.5 min：70% A, 0.5 ~ 10 min：70% A ~ 0% A, 10.0 ~ 10.1 min：0% A ~ 70% A, 10.1 ~ 14 min：70% A；Flow velocity：0.2 mL/min, the μ L of sampling volume 5；Ion gun：Using electron spray ionisation source；Scan mode：Cation scans；Detection mode：Multiple-reaction monitoring MRM；Electron spray Voltage：500 V；Dry temperature degree：325℃；Dry gas stream amount：6 L/min；Sheath temperature degree：380℃；Sheath throughput：10 L/ min；Capillary voltage：4000 V；（5）Draw standard curve and result of calculation：Aspiration step respectively（2）It is variant in the standard working solution series of preparation Strength solution carries out LC-MS/MS analyses, in step（4）Under the instrument parameter of determination, with 12 kinds of mycotoxin quota ion peaks face Product carries out linear regression to the mass concentration corresponding to it, obtains the standard working curve of each target compound；Aspiration step again （3）The sample solution of preparation carries out LC-MS/MS analyses, in step（4）Under the instrument parameter of determination, 12 kinds of mycotoxins are obtained Quota ion peak area, regression equation is substituted into, the concentration of 12 kinds of mycotoxins in sample solution is calculated.
- 2. the method according to claim 1 for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy, it is characterised in that：It is described Step（1）Aflatoxin mix mark be by aflatoxin B1, aflatoxin B 2, aflatoxin G 1, aflatoxin G2 is formed.
- 3. the method according to claim 1 for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy, it is characterised in that：It is described Step（1）Standard liquid be containing internal standard substance13C34Fumonisin B1 and13C17The solution of aflatoxin B1,13C34Lie prostrate horse Toxin B1 and13C17The concentration of aflatoxin B1 is respectively 20 μ g/mL.
- 4. the method according to claim 1 for detecting 12 kinds of mycotoxin concentrations in the tobacco leaf that goes mouldy, it is characterised in that：It is described Step（1）In methanol be chromatographically pure.
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| CN106442817A (en) * | 2016-11-30 | 2017-02-22 | 无锡艾科瑞思产品设计与研究有限公司 | Method for detecting mold in food |
| CN106770789B (en) * | 2017-01-16 | 2020-04-10 | 东北农业大学 | Ultra-high performance liquid chromatography method for simultaneously detecting contents of aflatoxin B1 and M1 in liver, kidney and chicken of broiler chicken |
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| CN113219092A (en) * | 2021-04-29 | 2021-08-06 | 中国烟草总公司湖北省公司 | Method for simultaneously measuring multiple aflatoxins in tobacco leaves by dispersion liquid-liquid microextraction-high performance liquid chromatography-tandem mass spectrometry |
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| CN103543221A (en) * | 2013-09-30 | 2014-01-29 | 王加启 | Method for simultaneously detecting multiple mycotoxins in milk |
| CN103713065B (en) * | 2014-01-06 | 2015-09-16 | 上海市农业科学院 | A kind of method simultaneously detecting multiple mycotoxin |
| CN104535664B (en) * | 2014-03-31 | 2016-03-16 | 中华人民共和国北京出入境检验检疫局 | A kind of method simultaneously detecting multiple mycotoxin in sesame paste |
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| CN106018648A (en) | 2016-10-12 |
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